CN102590377A - Method for synchronously measuring content of impurities of lithium phosphate and lithium pyrophosphate of lithium ferrous phosphate anode material - Google Patents
Method for synchronously measuring content of impurities of lithium phosphate and lithium pyrophosphate of lithium ferrous phosphate anode material Download PDFInfo
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- 239000012535 impurity Substances 0.000 title claims abstract description 30
- 229910001386 lithium phosphate Inorganic materials 0.000 title claims abstract description 25
- TWQULNDIKKJZPH-UHFFFAOYSA-K trilithium;phosphate Chemical compound [Li+].[Li+].[Li+].[O-]P([O-])([O-])=O TWQULNDIKKJZPH-UHFFFAOYSA-K 0.000 title claims abstract description 25
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 24
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title abstract description 15
- 239000010405 anode material Substances 0.000 title abstract description 4
- MVGWWCXDTHXKTR-UHFFFAOYSA-J tetralithium;phosphonato phosphate Chemical compound [Li+].[Li+].[Li+].[Li+].[O-]P([O-])(=O)OP([O-])([O-])=O MVGWWCXDTHXKTR-UHFFFAOYSA-J 0.000 title abstract 5
- 229940116007 ferrous phosphate Drugs 0.000 title abstract 2
- 229910000155 iron(II) phosphate Inorganic materials 0.000 title abstract 2
- SDEKDNPYZOERBP-UHFFFAOYSA-H iron(ii) phosphate Chemical compound [Fe+2].[Fe+2].[Fe+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O SDEKDNPYZOERBP-UHFFFAOYSA-H 0.000 title abstract 2
- 239000000463 material Substances 0.000 claims abstract description 23
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims abstract description 22
- 229940005657 pyrophosphoric acid Drugs 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 230000002378 acidificating effect Effects 0.000 claims abstract description 14
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 11
- 239000010452 phosphate Substances 0.000 claims abstract description 11
- 238000004255 ion exchange chromatography Methods 0.000 claims abstract description 4
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 18
- 239000010406 cathode material Substances 0.000 claims description 12
- 239000000523 sample Substances 0.000 claims description 11
- 235000011180 diphosphates Nutrition 0.000 claims description 10
- 150000002500 ions Chemical class 0.000 claims description 10
- 229940048084 pyrophosphate Drugs 0.000 claims description 10
- 229910052493 LiFePO4 Inorganic materials 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000003556 assay Methods 0.000 claims description 7
- 208000030208 low-grade fever Diseases 0.000 claims description 7
- 230000001360 synchronised effect Effects 0.000 claims description 7
- HNSDLXPSAYFUHK-UHFFFAOYSA-N 1,4-bis(2-ethylhexyl) sulfosuccinate Chemical compound CCCCC(CC)COC(=O)CC(S(O)(=O)=O)C(=O)OCC(CC)CCCC HNSDLXPSAYFUHK-UHFFFAOYSA-N 0.000 claims description 6
- 238000004587 chromatography analysis Methods 0.000 claims description 5
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 238000012360 testing method Methods 0.000 claims description 5
- 239000012496 blank sample Substances 0.000 claims description 3
- 238000010828 elution Methods 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000011248 coating agent Substances 0.000 abstract 1
- 238000000576 coating method Methods 0.000 abstract 1
- 238000000691 measurement method Methods 0.000 abstract 1
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 6
- 239000011574 phosphorus Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 244000248349 Citrus limon Species 0.000 description 3
- 235000005979 Citrus limon Nutrition 0.000 description 3
- NJXVPIZBZLQQPB-UHFFFAOYSA-N N1=CC=CC2=CC=CC=C12.[Mo] Chemical compound N1=CC=CC2=CC=CC=C12.[Mo] NJXVPIZBZLQQPB-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 150000002576 ketones Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 239000005955 Ferric phosphate Substances 0.000 description 1
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229940010552 ammonium molybdate Drugs 0.000 description 1
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 description 1
- 239000011609 ammonium molybdate Substances 0.000 description 1
- 235000018660 ammonium molybdate Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- REKWWOFUJAJBCL-UHFFFAOYSA-L dilithium;hydrogen phosphate Chemical compound [Li+].[Li+].OP([O-])([O-])=O REKWWOFUJAJBCL-UHFFFAOYSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940032958 ferric phosphate Drugs 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- -1 phosphate radical Chemical class 0.000 description 1
- DHRLEVQXOMLTIM-UHFFFAOYSA-N phosphoric acid;trioxomolybdenum Chemical compound O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.OP(O)(O)=O DHRLEVQXOMLTIM-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a method for synchronously measuring the content of impurities of lithium phosphate and lithium pyrophosphate of a lithium ferrous phosphate anode material, in particular to a method for measuring the content of lithium phosphate and lithium pyrophosphate of a carbon-coating lithium iron phosphate anode material by an ion chromatography method. The method comprises the following steps: (1) extracting the impurities of lithium phosphate and lithium pyrophosphate from the lithium iron phosphate material by using a weakly acidic water solution with pH of 5.0-7.0; and (2) measuring the content of phosphate radicals and pyrophosphoric acid radicals of the extracting liquid by the ion chromatography method, and performing simple conversion to obtain the content of the impurities of lithium phosphate and lithium pyrophosphate in the material. The measurement method has the advantages of simplicity in operation, short analysis time, sensitivity and accuracy, small using amount of the reagent and low pollution, and provides an effective method for detecting the content of impurities of the lithium iron phosphate material.
Description
Technical field
The present invention relates to the assay method of impurity content in a kind of anode material for lithium-ion batteries, impurity lithium phosphate and pyrophosphoric acid Measurement of lithium content method in particularly a kind of lithium iron phosphate cathode material.
Background technology
Lithium ion battery is than general battery; Have sparking voltage height, specific energy high, have extended cycle life, advantages such as self-discharge rate is low, memory-less effect; Thereby extensively apply in various portable type electronic products and the communication tool, and progressively developed into the electrical source of power of electric motor car.At present, the lithium ion battery material that is used for electrokinetic cell mainly contains LiMn2O4, ternary material and LiFePO4.Lithium iron phosphate positive material can take off embedding Li reversiblely
+, environmental pollution is little, raw material sources are abundant, specific storage is high and good cycle, is the desirable positive electrode of lithium ion battery.Large-scale portable power source is low to the specific storage density requirements of material, and is strict to material price, security performance and environmental-protecting performance, and these all meet LiFePO
4Characteristics, make LiFePO
4Become the preferred material of power lithium-ion battery.
In the production run of reality; Because the ratio of Li, Fe, P might not reach the desired proportions value when producing design in the finished product lithium iron phosphate material; Under the influence of production technology and production run; Tend to exist some impurity such as lithium phosphate and pyrophosphoric acid lithium etc. in the LiFePO 4 material, the existence of these impurity will inevitably have influence on the performance of LiFePO 4 material, therefore needs effective measurement means to come the content of checked for impurities.And, have only the analytical approach of phosphorus in the LiFePO4, iron, lithium and carbon content at present also not to the concrete detection method of impurities content in the LiFePO 4 material of producing; And the detection of phosphate radical and pyrophosphate at present mainly adopts is AAS; Be based on phosphate radical and pyrophosphate and ammonium molybdate and form coloured complex compound; Under the light wave of certain wavelength, absorption is arranged; Utilize spectrophotometric instrumentation absorbance, obtain the content of phosphate radical and pyrophosphate again with the typical curve comparison.And during with the above-mentioned impurity content of AAS separation detection, have that reagent dosage is big, environmental pollution is big, the loaded down with trivial details problem such as time-consuming of method, the sensitivity of detection is also not high enough,, is difficult to accurately detect when extremely low like the phosphate radical in the sample and pyrophosphate content.In addition, quinoline molybdenum lemon ketone method can only working sample in total phosphorus content, and can not distinguish different phosphorus containing components and content.The present invention is with the content of impurity lithium phosphate and pyrophosphoric acid lithium in the chromatography of ions synchronous detection ferric phosphate lithium cell material.
Summary of the invention
Technical matters to be solved by this invention is to propose impurity lithium phosphate and pyrophosphoric acid Measurement of lithium content method in a kind of lithium iron phosphate positive material.
The present invention solves the problems of the technologies described above through following technical scheme:
The synchronous assay method of impurity lithium phosphate and pyrophosphoric acid lithium content is characterized in that in the lithium iron phosphate cathode material, may further comprise the steps:
(1) will be dissolved in fully stirring in the weakly acidic low-grade fever water with the lithium iron phosphate cathode material sample of measuring; Behind lixiviate 15-3min under the 35-75 ℃ of condition; Solution is filtered, collect filtrating, wherein; The mass volume ratio of tested LiFePO4 sample and slightly acidic water solution is 1:50-500 g/ml, and the pH value of slightly acidic water solution is 5.0-7.0;
The filtrating of (2) step (1) being extracted is diluted to suitable concentration with ultrapure water, and the solution after requiring to dilute is fit to measure with ion chromatograph;
(3) the slightly acidic water solution that does not add lithium iron phosphate cathode material of choosing identical extension rate is blank sample;
(4) use phosphate radical and pyrophosphate content in the extract after ion chromatography step (2) dilution then;
(5) peak area of phosphate radical that chromatography of ions is measured and pyrophosphate is brought typical curve into and is promptly obtained the two corresponding concentration, and calculating can obtain impurity lithium phosphate and pyrophosphoric acid lithium content in the material,
Used chromatograph is the U.S. DX-500 of a Dionex company type ion chromatograph, and test condition is: Dionex IonPac AS11 type; Moving phase is 5-100 mmol/L NaOH solution, gradient elution, and flow velocity is 1.8 mL/min; Suppressing electric current is 300 mA, electric conductivity detector.
The mass volume ratio of tested LiFePO4 sample and slightly acidic water solution is 1:150 g/ml in the step (1).
The temperature of the WS is 55 ℃ in the step (1).
The time of step (1) low-grade fever lixiviate is 15 min.
Impurity lithium phosphate and pyrophosphoric acid Measurement of lithium content method in the lithium iron phosphate positive material may further comprise the steps:
(1) use pH under the condition of low-grade fever, to extract lithium phosphate and pyrophosphoric acid lithium impurity in the LiFePO 4 material as the slightly acidic water solution of 5.0-7.0; The mass volume ratio of tested LiFePO4 sample and slightly acidic water solution is 1:50-500 g/ml, preferred 1:150 g/ml; The temperature of low-grade fever is 35-75 ℃, preferred 55 ℃; The time of low-grade fever is 10-30 min, preferred 15min; (2) extract is diluted to suitable concn, uses chromatography of ions (IC) to measure phosphate radical and pyrophosphate content in the extract again, can obtain impurity lithium phosphate and pyrophosphoric acid lithium content in the material through simple computation.
The faintly acid aqueous ph value is 6.6-6.9.
Theoretical foundation of the present invention is that lithium phosphate and pyrophosphoric acid lithium are dissolved in diluted acid and are slightly soluble in water, and LiFePO4 is insoluble to the more water-fast characteristic of diluted acid.
Impurity lithium phosphate and pyrophosphoric acid Measurement of lithium content method in the lithium iron phosphate positive material that the present invention proposes; Simple to operate, analysis time short, sensitive and accurate, reagent dosage is few and pollute few, can detect the effective means that provide for the impurity content of lithium iron phosphate positive material.
Embodiment
Further specify technical scheme of the present invention below.
Impurity lithium phosphate and pyrophosphoric acid Measurement of lithium content method in a kind of lithium iron phosphate cathode material specifically comprise the steps: to take by weighing 0.2034 g carbon-coated LiFePO 4 for lithium ion batteries sample, add the WS of 20 ml pH=6.7, and 55 ℃ are heated 15 min down.With the glass sand core funnel with liquid filtering after, fully wash filter residue with ultrapure water, collect filtrating, the filtrating of collecting is transferred to constant volume in the 50 ml volumetric flasks, get dilution 25 μ L; The slightly acidic water solution that does not add LiFePO4 choosing identical extension rate is blank sample, on the U.S. DX-500 of Dionex company type ion chromatograph, tests, and test condition is: Dionex IonPac AS11 type; Moving phase is 5-100 mmol/L NaOH solution, gradient elution, and flow velocity is 1.8 mL/min; Suppressing electric current is 300 mA, electric conductivity detector.The phosphate radical that chromatography of ions is measured and the peak area of pyrophosphate are brought typical curve into and promptly obtained the two corresponding concentration, and be as shown in the table:
? | The pyrophosphoric acid lithium | Lithium phosphate |
Measured matter content (wt%) in the dilution | 0.35 | 36.54 |
Measured matter content (wt%) in LiFePO 4 after calculating | 0.001015 | 0.105966 |
Test figure
In order to verify the inventive method result's accuracy, adopt quinoline molybdenum lemon ketone method promptly through in acid medium, PO
4 3-Generate yellow phosphomolybdic acid quinoline deposition with the reaction of quinoline molybdenum lemon ketone precipitation agent; Quality through deposition comes the principle of the total phosphorus content in the calculation sample to measure total phosphorus content in the above-mentioned dilution; Be 9.84wt%; The total phosphorus content 9.87wt% that the lithium phosphate content that this value and above-mentioned IC measure obtains after converting is very identical, this explanation the present invention based on the selective dissolution theory be feasible.
This shows impurity lithium phosphate and pyrophosphoric acid Measurement of lithium content method in the lithium iron phosphate positive material that the present invention proposes, simple to operate, analysis time short, can realize the analysis of PPM level impurity content.
Claims (4)
1. the synchronous assay method of impurity lithium phosphate and pyrophosphoric acid lithium content in the lithium iron phosphate cathode material is characterized in that, may further comprise the steps:
(1) will be dissolved in fully stirring in the weakly acidic low-grade fever water with the lithium iron phosphate cathode material sample of measuring; Behind lixiviate 15-3min under the 35-75 ℃ of condition; Solution is filtered, collect filtrating, wherein; The mass volume ratio of tested LiFePO4 sample and slightly acidic water solution is 1:50-500 g/ml, and the pH value of slightly acidic water solution is 5.0-7.0;
The filtrating of (2) step (1) being extracted is diluted to suitable concentration with ultrapure water, and the solution after requiring to dilute is fit to measure with ion chromatograph;
(3) the slightly acidic water solution that does not add lithium iron phosphate cathode material of choosing identical extension rate is blank sample;
(4) use phosphate radical and pyrophosphate content in the extract after ion chromatography step (2) dilution then;
(5) peak area of phosphate radical that chromatography of ions is measured and pyrophosphate is brought typical curve into and is promptly obtained the two corresponding concentration, and calculating can obtain impurity lithium phosphate and pyrophosphoric acid lithium content in the material,
Used chromatograph is the U.S. DX-500 of a Dionex company type ion chromatograph, and test condition is: Dionex IonPac AS11 type; Moving phase is 5-100 mmol/L NaOH solution, gradient elution, and flow velocity is 1.8 mL/min; Suppressing electric current is 300 mA, electric conductivity detector.
2. the synchronous assay method of impurity lithium phosphate and pyrophosphoric acid lithium content in the lithium iron phosphate cathode material according to claim 1 is characterized in that: the mass volume ratio of tested LiFePO4 sample and slightly acidic water solution is 1:150 g/ml in the step (1).
3. the synchronous assay method of impurity lithium phosphate and pyrophosphoric acid lithium content in the lithium iron phosphate cathode material according to claim 1 is characterized in that: the temperature of the WS is 55 ℃ in the step (1).
4. the synchronous assay method of impurity lithium phosphate and pyrophosphoric acid lithium content in the lithium iron phosphate cathode material according to claim 1 is characterized in that: the time of step (1) low-grade fever lixiviate is 15 min.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103575679A (en) * | 2013-11-15 | 2014-02-12 | 合肥国轩高科动力能源股份公司 | Method for detecting content of lithium metasilicate in lithium ferrous silicate cathode material |
CN104730162A (en) * | 2015-03-13 | 2015-06-24 | 安徽皖仪科技股份有限公司 | Ion chromatograpy method for detecting trace anion content in iron phosphate |
CN106596831A (en) * | 2017-01-23 | 2017-04-26 | 合肥国轩高科动力能源有限公司 | Lithium ion battery shell lithium salt residue quantitative detection method |
CN110785386A (en) * | 2017-08-24 | 2020-02-11 | 株式会社住田光学玻璃 | Precursor glass of lithium-phosphorus composite oxide and method for producing same, method for producing crystallized glass of precursor of lithium-phosphorus composite oxide, and lithium-phosphorus composite oxide powder and method for producing same |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103575679A (en) * | 2013-11-15 | 2014-02-12 | 合肥国轩高科动力能源股份公司 | Method for detecting content of lithium metasilicate in lithium ferrous silicate cathode material |
CN103575679B (en) * | 2013-11-15 | 2016-06-22 | 合肥国轩高科动力能源有限公司 | The detection method of lithium metasilicate impurity content in ferrous silicate lithium anode material |
CN104730162A (en) * | 2015-03-13 | 2015-06-24 | 安徽皖仪科技股份有限公司 | Ion chromatograpy method for detecting trace anion content in iron phosphate |
CN106596831A (en) * | 2017-01-23 | 2017-04-26 | 合肥国轩高科动力能源有限公司 | Lithium ion battery shell lithium salt residue quantitative detection method |
CN110785386A (en) * | 2017-08-24 | 2020-02-11 | 株式会社住田光学玻璃 | Precursor glass of lithium-phosphorus composite oxide and method for producing same, method for producing crystallized glass of precursor of lithium-phosphorus composite oxide, and lithium-phosphorus composite oxide powder and method for producing same |
US11345597B2 (en) * | 2017-08-24 | 2022-05-31 | Sumita Optical Glass, Inc. | Precursor glass of lithium phosphorus complex oxide and method of producing same, method of producing precursor crystallized glass of lithium phosphorus complex oxide, and lithium phosphorus complex oxide powder and method of producing same |
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Free format text: CORRECT: APPLICANT; FROM: HEFEI GUOXUAN HIGH-TECH POWER ENERGY CO., LTD. TO: HEFEI GUOXUAN HIGH-TECH POWER ENERGY CO., LTD. |
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RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120718 |